About the Core
The Bioanalytical Core serves as an analytical resource for the research community by providing services for the detection and quantification of small molecules, and elements in user samples.
The core is located in Biomedical Research Building II, for LC-MS-based analysis of small molecules managed by Dr. Eryn Matich, Milesh Joseph and and Dr. Amar Singh.. The ICP-MS for elemental analysis is located in the Winthrop P Rockefeller Cancer Institute (WPRCI) and managed by Dr. Shelbie Stahr. Dr. Ping-Ching Hsu (PHsu@uams.edu) is the Core Director. Please reach out to them for any questions or inquiries or schedule a brief consultation to discuss your project or research needs.
Overview of Services
The core is equipped with mass spectrometers with routine maintenance, calibration, tuning, and cleaning to ensure optimal instrument performance and high-quality data. Our services provided include:
- Consultation and communication with users: We will work with each investigator to discuss the goal of the project, suggest an experimental design according to the research plans, provide updates on the progress of each project, and share study data/results in a timely manner.
- Method development and protocol testing: Methods and protocols not previously established in the core will need to be tested and developed before running precious research samples, even for methods in any published protocols. To do this, we will work with the user to determine the chemicals and sample types of interest, review the literature and test the published protocols.
- Sample preparation for data acquisition: To detect (and quantify) chemicals with minimal noise signals, most samples need some form of preparation or extraction depending on the bio-specimen used. Methods needed may include basic sample clean-up, liquid-liquid extraction, sonication, bead milling/homogenization, solid phase extraction (SPE), or microwave digestion.
- Running analytical instrumentation: Extracted/prepared samples will be injected to the designated instrumentation based on research needs for data acquisition. Multiple quality assurance (QA) and quality control (QC) procedures are implemented to monitor the instrument’s performance during the run.
- Initial and final data processing: Following data acquisition on the instrumentation, initial and final data will be processed using the associated software packages on the data acquisition computer. Following this, we will securely transfer data to our dedicated data storage and analysis computer and share with the user via online drive or email.
- Grant and manuscript writing: When needed, the core will assist in writing sections related to the core services in grant proposals and research papers.
List of example assays offered by the core:
- Therapeutics such as Doxirubicin, GGTi-2133 and a novel TGF beta inhibitor
- Endogenous compounds such as basic nucleosides, nucleotides, nucleoside derivatives (deoxyguanosine, iodo-deoxyuridine, chloro-deoxyuridine), S-adenosylmethionine, S-adenosylhomocystine, and tocotrienol.
- Elemental analysis such as arsenic, gold, copper, chromium, zinc, selenium, lead, nickel, platinum, iron, and rubidium.
Amount of each matrix needed for core analysis:
- Whole blood, serum, plasma, urine, saliva, cells (pellets, lysates): 100 µL (500 µL for ICP-MS)
- Tissue and other solid sample types: 100 mg
Instrumentation
Instrumentation associated with the Bioanalytical Core includes the following:
UHPLC – Triple Quad MS
- Agilent Infinity II 1260 ultra-high performance liquid chromatography (UHPLC) with column manager, autosampler, binary pump, high dynamic range Diode Array Detector (DAD)
- Agilent Ultivo triple quadrupole (TQ) MS
The UHPLC – triple quad MS is the primary instrumentation in the core for targeted data acquisition.
HPLC – Single Quad MS
- Waters Acquity high-performance liquid chromatography (HPLC) with column heater, sample manager, and binary solvent manager
- Waters Photo Diode Array (PDa)/ Quadrupole Dalton (QDa) mass selective detector (MSD) MS
The HPLC-single quad MS is an additional instrument for targeted data acquisition.
HPLC – HR-MS
- Waters Acquity high-performance liquid chromatography (HPLC) with column heater, sample manager, and binary solvent manager
- Waters Micromass Premier quadrupole – time of flight (Q-ToF) MS, a high resolution-mass spectrometer (HR-MS)
The HPLC – is the primary instrumentation in the core for high-resolution drug discovery data acquisition and general untargeted data acquisition.
ICP-MS (with or without UHPLC)
- Thermo Fisher Scientific iCAP RQ inductively coupled plasma mass spectrometer (ICP-MS).
- Coupled with an ESI AutoSampler 4DX for accurate and precise sampling, high sample throughput, and automated and customizable rinse configurations.
- Optional microwave digestion with CEM MARS6 Microwave Digestion System is available for sample preparation.
- Optional Thermo Fisher Scientific Vanquish Flex UHPLC System coupled to the ICP-MS for speciation analysis.
The ICP-MS is the primary instrumentation in the core for trace element quantification as low as parts per trillion. ICP-MS protocols specialized in heavy metal analyses have been established for several matrices including saliva, urine, plasma, as well as various tissues. Current methods include the following analytes: 51V, 52Cr, 55Mn, 56Fe, 60Ni, 63Cu, 64Zn, 65Cu, 75As, 78Se, 80Se, 85Rb, 111Cd, 190Pt, 192Pt, 194Pt, 195Pt, 196Pt, 197Au, 198Pt, 206Pb, 207Pb, 208Pb.
GC-MS (user availability coming soon!)
- Agilent 7890A gas chromatography (GC)
- Agilent 5975C inert XL single quadrupole/mass selective detector (MSD, triple-axis detector) with Agilent 7693 autosampler
The GC-MS will be the primary instrumentation in the core for targeted volatile and therapeutic molecule data acquisition.
Until this specific instrument is operational we are collaborating with David Church at the Institute on Aging to run users’ samples on their GC-MS.
Other Research Equipment
The core has various other pieces of research equipment used for sample storage, preparation, and data analysis. Temporary sample storage can be in the fridge/freezer at 4°C, -20°C, or -80°C. For various types of sample preparation, we have a scale, incubator, oven, shaker, vortex, water bath sonicator, bullet blender, TissueLyzer, Bertin Precellys homogenizer with Cryolys, solid phase extraction manifolds, centrifuge, SpeedVac concentrator, and CEM MARS6 microwave digestion.
Data/Results Storage and Analysis
A dedicated data storage and analysis computer with 64 GB RAM and 1 TB of hard drive space is in place in the Biomed Lab. Software packages for data analysis and manuscript/presentation editing are available including ACD Labs, Partek Genomics Suite, GIMP, EndNote, Adobe Acrobat Pro, and Microsoft Office Professional. Data will be stored in an online drive (UAMS Box, OneDrive, or SharePoint), and users will be given access.
Acknowledgment/ Citation/ Training
All users agree to acknowledge the use of the Bioanalytical Core (see acknowledgment language below) in scholarly work such as publications, presentations, and posters and provide a copy of this work. If a new or modified method was developed for your research project or you feel that we contributed in a significant manner, the core will also help the users write sections related to the core services in grant proposals and research papers.
To acknowledge the core, please state: Research reported in this publication was supported by the UAMS Bioanalytical Core (NIH P20 GM109005).
Contacts
Core Director
Ping-Ching Hsu, PhD
Email: PHsu@uams.edu
Small molecules
Eryn Matich, PhD
Email: EMatich@uams.edu
Milesh Joseph, MS
Email: MThattasseryjoseph@uams.edu
Amar Singh, PhD
Email: ASingh@uams.edu